反応 #62746

反応方程式

sodium methoxide

3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile

→

yellow oil

収率 62.2%

3-(7,8-Dimethoxy-2H-1-benzopyran-5-yl)-2-dimethoxymethylpropanenitrile

収率 62.2%

溶媒

water

methanol

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux for 24 hr
3. 3
   温度to cool
4. 4
   抽出The resultant mixture was extracted with toluene (1×200 mL and 2×100 mL)
5. 5
   抽出The combined toluene portions were extracted with water (3×100 mL)
6. 6
   乾燥dried over magnesium sulfate
7. 7
   濃縮The toluene solution was concentrated
8. 8
   その他leaving a brown oil which
9. 9
   workup.DISTILLATIONwas distilled under reduced pressure

実験手順

A mixture of sodium methoxide (8.86 g, 0.164 mole), and 3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile (Example 37A, 23.1 g, 0.080 mole) in methanol (60 mL) was heated at reflux for 24 hr, allowed to cool and diluted with water (200 mL). The resultant mixture was extracted with toluene (1×200 mL and 2×100 mL). The combined toluene portions were extracted with water (3×100 mL) and dried over magnesium sulfate. The toluene solution was concentrated leaving a brown oil which was distilled under reduced pressure to give 15.9 g (62%) of a yellow oil which was used without further purification.

出典